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Determination method of oritavancin intermediate impurity 4-chlorobiphenyl and 4,4-dichlorobiphenyl content

A technology for oritavancin and determination method, which is applied to measurement devices, instruments, scientific instruments, etc., can solve the problems of interference detection, insufficient sensitivity, easy high temperature degradation of oritavancin intermediate side chains, etc., and achieves improved accuracy. , Improve sensitivity, good effect of impurity recovery

Active Publication Date: 2022-04-08
HANGZHOU HUADONG MEDICINE GRP PHARMA RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to overcome the insufficient sensitivity of the prior art to detect oritavancin intermediate impurities 4-chlorobiphenyl and 4,4-dichlorobiphenyl, and the side chains of oritavancin intermediates are easy to degrade at high temperature, thereby interfering with detection question

Method used

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  • Determination method of oritavancin intermediate impurity 4-chlorobiphenyl and 4,4-dichlorobiphenyl content
  • Determination method of oritavancin intermediate impurity 4-chlorobiphenyl and 4,4-dichlorobiphenyl content
  • Determination method of oritavancin intermediate impurity 4-chlorobiphenyl and 4,4-dichlorobiphenyl content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] 1. Detection

[0058] A. Preparation of the test solution:

[0059] Accurately weigh 0.05 g of the oritavancin side chain sample shown in formula I into a stoppered test tube, add 4 mL of acetonitrile, shake to dissolve the sample completely, then precisely add 5.0 mL of n-hexane, shake fully, and let stand Layering, take the upper n-hexane layer and set aside;

[0060] B. Preparation of reference substance solution:

[0061] Accurately weigh an appropriate amount of 4-chlorobiphenyl and 4,4-dichlorobiphenyl, mix and dissolve with N,N-dimethylformamide, quantitatively dilute to make a solution of 20 μg / mL each, and use it as the mother solution of the reference substance; Measure 0.01mL, 0.025mL, 0.04mL, 0.05mL and 0.06mL of the mother liquor of the reference substance, put them into a stoppered test tube, add 4mL of acetonitrile, shake and mix evenly, then precisely add 5.0mL of n-hexane, shake fully, and let stand to separate layer, take the upper n-hexane layer as...

Embodiment 2

[0069] A. Preparation of the test solution

[0070] Accurately weigh 0.1 g of the oritavancin side chain sample shown in formula I into a stoppered test tube, add 4 mL of acetonitrile, shake to dissolve the sample completely, then precisely add 5.0 mL of n-hexane, shake fully, and let stand Layering, take the upper n-hexane layer and set aside;

[0071] Steps B and C refer to Example 1.

[0072] According to the above conditions, three batches of test solution were detected, and the results are shown in Table 2.

[0073] Table 2:

[0074]

[0075]

Embodiment 3

[0077] A. Preparation of the test solution

[0078] Accurately weigh 0.05 g of the oritavancin side chain sample shown in formula I into a stoppered test tube, add 5 mL of acetonitrile, shake to dissolve the sample completely, then precisely add 5.0 mL of n-hexane, shake fully, and let stand Layering, take the upper n-hexane layer and set aside;

[0079] Steps B and C refer to Example 1.

[0080] According to the above conditions, three batches of test solution were detected, and the results are shown in Table 3.

[0081] table 3:

[0082]

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Abstract

The invention provides a method for determining the content of oritavancin intermediate impurities 4-chlorobiphenyl and 4,4-dichlorobiphenyl. By adopting acetonitrile and n-hexane double organic phase extraction system to separate oritavancin side chain shown in formula I and intermediate impurity 4-chlorobiphenyl shown in formula II, intermediate impurity 4 shown in formula III , 4‑dichlorobiphenyl, and the impurity content was detected by gas chromatography‑mass spectrometry. This method avoids the interference of the oritavancin intermediate side chain on the test results, has high sensitivity and accuracy, is simple to operate, and is suitable for industrial production applications. It provides a basis for the quality control of oritavancin products, thereby ensuring the quality of drugs .

Description

technical field [0001] The invention belongs to the technical field of drug detection and analysis, in particular to a method for determining the content of oritavancin intermediate impurities 4-chlorobiphenyl and 4,4-dichlorobiphenyl. Background technique [0002] Oritavancin (trade name: Orbactiv, generic name: oritavancin), FDA approved Oritavancin injection on August 7, 2014 for use by sensitive Gram-positive bacteria (including methicillin-resistant Staphylococcus aureus, MRSA ) for the treatment of adult patients with acute bacterial skin and skin structure infections (ABSSSIs). The oritavancin side chain process shown in formula I is: [0003] [0004] This reaction can produce 4-chlorobiphenyl as shown in formula II and 4,4-dichlorobiphenyl as shown in formula III, these two kinds of impurity belong to halogenated aromatic ring genotoxic warning structure, must be to this type of gene Toxic impurities shall be controlled by formulating scientific methods. [00...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/88G01N30/06G01N2030/8872G01N2030/884G01N2030/025G01N2030/062
Inventor 陈阳张立波陈蓓雍春何廖琳武天浩李玲玲
Owner HANGZHOU HUADONG MEDICINE GRP PHARMA RES INST
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